Calibration of δ17O and 17Oexcess values of three international standards: IAEA‐603, NBS19 and NBS18

Barkan, Eugeni; Affek, Hagit P.; Luz, Boaz; Bergel, S.; Voarintsoa, Ny Riavo G.; Musan, Israela

doi:10.1002/rcm.8391

Cited by 29 publications

(48 citation statements)

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“…For high accuracy δ 13 C determinations, the similarity of the 17 O/ 18 O relationship in IAEA‐603‐CO 2 and NBS19‐CO 2 cannot be taken for granted. Recently, δ 17 O values for IAEA‐603, NBS19 and NBS18 were measured with high accuracy 43 . In this study, CO 2 was extracted from a few milligrams of carbonate RMs by reaction with H 3 PO 4 in the same way as used at the IAEA (acid reaction at 25°C, see more details in Barkan et al 43 ).…”

Section: Resultsmentioning

confidence: 95%

“…Uncertainties are given at k = 1. The17 O excess values in Barkan et al43 for NBS19 and IAEA-603 are representative (several ampoules of each RM) and self-consistent. Small negative17 O deviations of carbonate-based CO 2 from the reference line (VSMOW line with λ = 0.528) reflect the position of the VPDB-CO 2 oxygen triple-isotope scale relative to the respective VSMOW scale.…”

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confidence: 90%

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Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ¹³C and δ¹⁸O determination

Assonov

Groening

Fajgelj

et al. 2020

Rapid Comm Mass Spectrometry

107

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Rationale NBS19 carbonate, a primary reference material (RM) for the Vienna Pee Dee Belemnite (VPDB) scale realisation introduced in 1987, was exhausted in 2009, and no primary RM was available for several years. This study describes the preparation and characterisation of a new RM, IAEA‐603 (Ca‐carbonate, calcite of marble origin), which shall serve as a new primary RM (replacement for NBS19) or primary calibrator aimed at the highest realisation of the VPDB scale for δ13C and δ18O values, including the VPDB‐CO2 δ18O scale. Methods IAEA‐603 preparation and characterisation (value transfer) against NBS19 were performed by addressing the major modern technical requirements for the production and characterisation of RMs (ISO Guide 35). IAEA‐603 was produced in a large quantity, and the first batch was sealed into ampoules (0.5 g) to ensure RM integrity during storage; four other batches were sealed for long‐term storage. The most accurate method of CO2 preparation for isotope mass spectrometry was used, namely carbonate–H3PO4 reaction under controlled conditions. Results The assigned values of δ13C = +2.460 ± 0.010‰ and δ18O = −2.370 ± 0.040‰ (k = 1) are based on a large number of analyses (~10 mg aliquots) performed at IAEA and address all the known uncertainty components. For aliquots down to 120 μg, the δ18O uncertainty remains unchanged but shall be doubled for δ13C. The uncertainty components considered are as follows: (a) material homogeneity (within and between the 5200 ampoules produced), (b) value assignment against NBS19, (c) storage effects and (d) effect of the 17O correction. Conclusions The new primary RM IAEA‐603 replaces NBS19 in its use as the highest calibrator for the VPDB δ13C and δ18O scale, including the VPDB‐CO2 δ18O scale. The use of IAEA‐603 will allow laboratories worldwide to establish consistent realisation of the scales for δ13C and δ18O values and metrological comparability of measurement results for decades. The VPDB scale definition based on NBS19 stays valid.

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Section: Resultsmentioning

confidence: 95%

mentioning

confidence: 90%

Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ¹³C and δ¹⁸O determination

Assonov

Groening

Fajgelj

et al. 2020

Rapid Comm Mass Spectrometry

107

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“…Differences reported by different laboratories should agree, even if the absolute values may differ. However, the difference 17 O(NBS19)-17 O(NBS18) reported by (Wostbrock et al, 2019) and (Fosu et al, 2020) is -0.050 ‰, whereas (Passey et al, 2014) and (Barkan et al, 2019) reported smaller differences, -0.037 ‰ and -0.019 ‰, respectively. Part of the difference may be due to sample preparation.…”

Section: Interlaboratory Comparisonmentioning

confidence: 85%

“…(Wostbrock et al, 2019) used a calcite fluorination method to extract CO2, the other studies measured the CO2 extracted from carbonate using H3PO4 acid digestion. The relative difference between 17 O(NBS18) and 17 O(IAEA603) (a replacement for NBS19) is reported as -0.042 ‰ by Sha et al, (2020) and -0.010 ‰ by (Barkan et al, 2019). The relative difference between the carbonate standards can be determined independently using the fragment technique developed in this PhD thesis (see below).…”

Section: Interlaboratory Comparisonmentioning

confidence: 95%

“…The most commonly used ref is 0.528, the value that is also used in this thesis (Sharp et al, 2018;Wostbrock et al, 2019;Passey et al, 2014;Landais et al, 2006;Meijer and Li, 1998;Barkan et al, 2019;Fosu et al, 2020;Schoenemann et al, 2013;Young et al, 2016a). This is the value that has been established for meteoric waters (Meijer and Li, 1998;Luz and Barkan, 2010), and the reason for using ref = 0.528 also for CO2 is that the carbon and hydrological cycle are connected via oxygen isotope exchange between water and CO2.…”

Section: Consensus In the Reference Slopementioning

confidence: 99%

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The effect of photosynthetic gas exchange on Δ17O of atmospheric CO2

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Rationale: Determination of 17 O directly from CO2 with traditional gas source isotope ratio mass spectrometry is not possible due to isobaric interference of 13 C 16 O 16 O on 12 C 17 O 16 O. The methods developed so far use either chemical conversion or isotope equilibration to determine 17 O of CO2. In addition, 13 C measurements require correction for the interference from 12 C 17 O 16 O on 13 C 16 O 16 O since it is not possible to resolve the two isotopologues. Methods: We present a technique to determine 17 O, 18 O and 13 C of CO2 from the fragment ions that are formed upon electron ionization in the ion source of the Thermo Scientific 253 Ultra High-Resolution Isotope Ratio Mass Spectrometer (hereafter 253 Ultra). The new technique is compared with the CO2-O2 exchange method and the 17 O-correction algorithm for 17 O and 13 C respectively. Results: Scale contractions for 13 C and 18 O are slightly larger for fragment ion measurements compared to molecular ion measurements. 17 O and 17 O of CO2 can be measured on the 17 O + fragment with an internal error that is a factor 1-2 above the counting statistics limit. The ultimate precision depends on the signal intensity and on the total time that the 17 O + beam is monitored; a precision of 14 ppm (parts per million) (standard error of the mean) was achieved in 20 hours at the University of Göttingen. The 17 O measurements with the O-fragment method agree with the CO2-O2 exchange method over a range of 17 O values of-0.3 to + 0.7 ‰. Conclusions: Isotope measurements on atom fragment ions of CO2 can be used as alternative method to determine the carbon and oxygen isotopic composition of CO2 without chemical processing or corrections for mass interferences.

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Characterisation of new reference materials IAEA‐610, IAEA‐611 and IAEA‐612 aimed at the VPDB δ¹³C scale realisation with small uncertainty

Assonov

Fajgelj

Hélie

et al. 2021

Rapid Comm Mass Spectrometry

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Rationale LSVEC, the second anchor Reference Material (RM) for the VPDB δ13C scale realisation, was introduced in 2006. In 2015, its δ13C value was found to be drifting and, in 2017, its use as an RM for δ13C was officially discontinued by IUPAC. New RMs of low uncertainty are needed. This paper describes the preparation and characterisation of IAEA‐610, IAEA‐611 and IAEA‐612 (calcium carbonate, of chemical origin) which shall serve as a set of RMs aimed at anchoring the VPDB scale at negative δ13C values. Methods The preparation and characterisation of IAEA‐610, IAEA‐611 and IAEA‐612 were performed by addressing the contemporary technical requirements for RM production and characterisation (ISO Guide 35:2017). The three RMs were produced in large quantities, and the first batch was sealed into ampoules (0.5 g) to ensure the integrity of the RM during storage; additional batches were sealed for long‐term storage. The most accurate method of CO2 preparation and stable isotope measurements was used, namely carbonate‐H3PO4 reaction under well‐controlled conditions combined with well‐tested stable isotope ratio mass spectrometry. Results The assigned values of δ13C and associated uncertainties are based on a large number of analyses (~10 mg aliquots) performed at IAEA and address all the known uncertainty components. For aliquots down to ~100 μg, the δ13C uncertainty is increased. The uncertainty components considered are as follows: (i) material homogeneity, (ii) value assignment against IAEA‐603, (iii) potential storage effects, (iv) effect of the 17O correction, and (v) mass spectrometer linearity and cross‐contamination memory in the ion source. Conclusions The new RMs IAEA‐610, IAEA‐611 and IAEA‐612 have been characterised on the VPDB δ13C scale in a mutually consistent way. The use of three RMs will allow a consistent realisation of the VPDB δ13C scale with small uncertainty to be established, and to reach metrological compatibility of measurement results over several decades.

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Calibration of δ¹⁷O and ¹⁷O_excess values of three international standards: IAEA‐603, NBS19 and NBS18

Cited by 29 publications

References 13 publications

Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ¹³C and δ¹⁸O determination

Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ¹³C and δ¹⁸O determination

The effect of photosynthetic gas exchange on Δ17O of atmospheric CO2

Characterisation of new reference materials IAEA‐610, IAEA‐611 and IAEA‐612 aimed at the VPDB δ¹³C scale realisation with small uncertainty

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Calibration of δ17O and 17Oexcess values of three international standards: IAEA‐603, NBS19 and NBS18

Cited by 29 publications

References 13 publications

Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ13C and δ18O determination

Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ13C and δ18O determination

The effect of photosynthetic gas exchange on Δ17O of atmospheric CO2

Characterisation of new reference materials IAEA‐610, IAEA‐611 and IAEA‐612 aimed at the VPDB δ13C scale realisation with small uncertainty

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Calibration of δ¹⁷O and ¹⁷O_excess values of three international standards: IAEA‐603, NBS19 and NBS18

Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ¹³C and δ¹⁸O determination

Preparation and characterisation of IAEA‐603, a new primary reference material aimed at the VPDB scale realisation for δ¹³C and δ¹⁸O determination

Characterisation of new reference materials IAEA‐610, IAEA‐611 and IAEA‐612 aimed at the VPDB δ¹³C scale realisation with small uncertainty